Preparation technology of cyclopentadiene or substituted cyclo pentadiene
A technology of cyclopentadiene and cyclopentenol, which is applied in the field of preparation technology of tetramethylcyclopentadiene, can solve the problems of difficult separation of reaction mixture and failure to reflect the actual yield of the target product, and achieve the goal of simplifying the process flow Effect
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Embodiment 1
[0025] After the reaction bottle has been fully inertly replaced, add 250ml of 1 ether and 17g of lithium aluminum tetrahydride in sequence, start stirring, and cool the mixture to 0°C. Under continuous stirring, add 45g (0.29mol) of Hydrogen-2,3,5,6 tetramethyl-γ-pyrone was slowly added dropwise into the reaction flask. After the addition, continue to stir for 0.5 hours, slowly raise the temperature to 25° C. and stir for 3 hours, slowly add acidic distilled water with pH=2 for hydrolysis. Then add 200ml of benzene and 62.8g of p-toluenesulfonic acid, and reflux for 12 hours in a boiling state to stop the reaction. The liquid in the reaction mixture was separated by decantation, the remaining solid was washed twice with ether and the washing liquid was mixed with the liquid obtained by decantation, neutralized to neutral with saturated sodium carbonate solution, the organic layer was washed twice with water, anhydrous magnesium sulfate Drying, filtration removes magnesium su...
Embodiment 2
[0027] After the reaction flask has been fully inertly replaced, add 1g of a mixture consisting of ferric chloride (0.2g) and copper chloride (0.8g), 250ml of 1 ether and 17g of lithium aluminum hydride in sequence, start stirring, and cool the mixture to 0 °C, under continuous stirring, slowly drop 45g (0.29mol) of 2,3,5,6-tetrahydro-2,3,5,6 tetramethyl-γ-pyrone into the reaction flask. The following steps are the same as in Example 1 to obtain 23.4 g of 1,2,3,4-tetramethylcyclopentadiene, (by feeding 2,3,5,6-tetrahydro-2,3,5,6 tetramethylcyclopentadiene Based on the moles of γ-pyrone) the yield was 66%.
Embodiment 3
[0036] With glacial acetic acid as a dehydrating agent, other processes are the same as in Example 2 to obtain 22.4 g of 1,2,3,4-tetramethylcyclopentadiene (with 2,3,5,6-tetrahydro-2,3, 5,6 moles of tetramethyl-γ-pyrone), the yield was 63.4%.
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